CN108054241B - A kind of enhancing CdIn2S4The method of optical absorption - Google Patents
A kind of enhancing CdIn2S4The method of optical absorption Download PDFInfo
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Abstract
The invention discloses a kind of enhancing CdIn2S4The method of optical absorption, comprising: in semiconductor CdIn2S4Middle doping nontransition metal atom Sn replaces part In atom, induces CdIn2S4Band gap generates interstitial impurity energy band, products therefrom CdIn2‑x Sn x S4, 0 in formula <x< 2, specifically: stoichiometrically weigh Cd, In, S and Sn raw material, in being warming up to 700-800 DEG C of reaction-sintered in quartz glass tube, furnace cooling after keeping the temperature 24-48 hours, then secondary response are sintered Vacuum Package to obtain the final product.For CdIn2S4The problem of some visible light can only be absorbed and utilized in semiconductor, be put forward for the first time and adulterated using nontransition metal Sn, induce CdIn2S4Impurity energy level generates, and regulates and controls by main semiconductor CdIn2S4Electronic band structure enhances CdIn2S4Optical absorption ability is good in photocatalysis, photovoltaic cell field application prospect.
Description
Technical field
The invention belongs to photoelectric semiconductor material technical fields, and in particular to a kind of enhancing CdIn2S4The side of optical absorption
Method.
Background technique
Solar energy as a kind of reproducible clean energy resource, have the advantages that it is resourceful, use without geographical restrictions, benefit
Electricity can be directly converted light into the photoelectric conversion effect of semiconductor, is a kind of important channel that people utilize solar energy.One
As semiconductor material can only be absorbed and utilized photon of the energy near band gap, energy is less than and the photon beyond band gap can not be by
Semiconductor directly utilizes, so as to cause energy loss.By semiconductor doping technique, intermediate level is introduced in semiconductor band gap
Or energy band, it can be realized the multi-absorption to sunlight, to preferably utilize solar spectrum energy.Too with impurity energy level
Positive energy battery theoretical limit efficiency is 63.1%, significantly the single tape battery theoretical limit efficiency 40.7% of beyond tradition
(Physical Review Letters, 1997,78(26):5014-5017)。
CdIn2S4Belong to ternary spinel structure compound, photoelectric properties are excellent, in photocatalysis, light emitting diode, photovoltaic
The fields such as battery have potential application prospect.CdIn2S4Optical band gap is relatively narrow compared with oxide (2.1eV), can preferably absorb
Visible light.In order to further increase CdIn2S4Optical absorption ability can be introduced in its band gap miscellaneous by element doping method
Mass-energy grade, to construct new optical absorption approach.Theoretical research discovery, Ti, V, Cr, Mn adulterate CdIn2S4It is mixed in will lead to
Matter band is formed, and is proved that the generation of impurity energy level can improve by the optical absorption spectra of main semiconductor and dopant material by calculating
Optical absorptive character (1, Physical Review B, 2010,81 (7): 075206；2,Journal of Alloys and
Compounds,2014, 591:22-28.)；In terms of experimental study, the Chinese patent of application number CN201611151273.1 is public
It has opened and has generated track in crystalline field using the 3d electronics of transition element Fe and cleave to form impurity energy level, found the half of doping
Conductor has wide spectrum Absorption Characteristics.
In conclusion in the prior art to CdIn2S4The improved method of optical absorption focus primarily upon it is transient metal doped,
And theoretical research is largely stayed in, with the serious disconnection of experiment；In addition, transition metal d electronics excessively local, is unfavorable for current-carrying
Son separation, new doping defect complex centre easy to form influences the practical photoelectric conversion performance of semiconductor.
Summary of the invention
For the drawbacks described above for overcoming the prior art, for CdIn2S4Asking for some visible light can only be absorbed and utilized in semiconductor
Topic, the purpose of the present invention is to provide a kind of enhancing CdIn2S4The method of optical absorption is mentioned for the first time using semiconductor doping technique
It is adulterated out using nontransition metal Sn, induces CdIn2S4Impurity energy level generates, and regulates and controls by main semiconductor CdIn2S4Electron energy band
Structure constructs new optical absorption approach to enhance its optical absorption ability.
The object of the invention is also to provide adulterate CdIn by Sn obtained by the above method2S4Semiconductor.
Above-mentioned purpose of the invention is achieved through the following technical solutions:
A kind of enhancing CdIn2S4The method of optical absorption, in semiconductor CdIn2S4Middle doping nontransition metal atom Sn, lures
Lead CdIn2S4Band gap in generate interstitial impurity energy band, wherein doping position is to replace described half with nontransition metal atom Sn
Conductor CdIn2S4Middle part In atom, the chemical molecular formula of products therefrom are CdIn2-xSnxS4, 0 < x < 2 in formula, including following step
It is rapid:
S1, according to the CdIn2-xSnxS4Stoichiometric ratio weigh Cd, In, S and Sn raw material, Vacuum Package is in quartzy glass
In glass pipe；
S2, quartz glass tube described in step S1 is placed in temperature programmed control Muffle furnace, it is slow with 2-5 DEG C/min of rate
Slowly 700-800 DEG C of reaction-sintered, furnace cooling after heat preservation 24-48 hours are warming up to；
S3, product after cooling described in step S2 is poured out and is ground, Vacuum Package is in quartz glass tube again, and
It is placed in temperature programmed control Muffle furnace, then 700-800 DEG C of reaction-sintered is to slowly warm up to 2-5 DEG C/min of rate, keep the temperature 24-48
It is regrind after furnace cooling after hour.
Further, Cd, In, S and Sn raw material described in step S1 include simple substance or binary compound, and purity is not low
In 99.99%.
Further, the interstitial impurity energy band has metallicity.
Further, the interstitial impurity energy band is formed by Sn-5s state and S-3p state hydridization.
Further, the doping content of nontransition metal atom Sn optimization is not more than 5at%.
One kind is by above-mentioned enhancing CdIn2S4The doping CdIn that the method for optical absorption obtains2S4Semiconductor, chemical molecular formula
For CdIn2-xSnxS4, wherein 0 < x < 2.
In one embodiment of the invention, Cd, In, S and Sn raw material is simple substance.
In another embodiment of the present invention, Cd, In, S and Sn raw material is binary compound.
On the basis of common knowledge of the art, above-mentioned each optimum condition can be in any combination up to each preferable reality of the present invention
Example；In addition the raw materials and reagents used in the present invention are unless otherwise stated commercially available or are conventional selection.
CdIn is adulterated in the present invention2S4In the characterization method of semiconductor, structure characterizes (XRD) using X ray diffracting spectrum,
Elemental analysis is measured (EDX) using energy disperse spectroscopy, and Determination of Different Valence States is characterized using photoelectron spectroscopy (XPS), ultraviolet-visible-near-infrared
Absorption spectrum measures on Hitachi U4100UV-Vis-NIR spectrophotometer.
Present invention firstly provides adulterating using nontransition metal Sn, CdIn is induced2S4Impurity energy level generates, the mechanism of formation
It is significantly different with bridging atom doping, replace part In atom with foreign atom Sn, Sn element has 5s5p electron configuration, S tool
Have a 3s3p electron configuration, Sn atom 5s electronics can with S3p electronics hydridization bonding around, thus in the band gap by main semiconductor
The new energy band of middle building.
Compared with prior art, the positive effect of the present invention is that:
(1)CdIn2S4Belong to ternary spinel structure compound, CdIn2S4Optical band gap is relatively narrow compared with oxide (2.1eV),
Some visible light can only be absorbed and utilized, the above method is in enhancing CdIn in the present invention2S4While optical absorption ability, significantly mention
High CdIn2S4Photoelectric conversion efficiency, the fields such as photocatalysis, photovoltaic cell have potential application prospect.
(2) CdIn is adulterated in the present invention2S4The UV-visible-near infrared absorption of semiconductor can observe two suctions
Side is received, optical absorption ability is remarkably reinforced, and further proves that nontransition metal Sn doping can effectively enhance CdIn2S4Optics
Absorbability.
Detailed description of the invention
Fig. 1 is CdIn2-xSnxS4(x=0,0.05,0.1) XRD spectrum of series of samples；
Fig. 2 is CdIn1.9Sn0.1S4EDX elemental analysis map；
Fig. 3 is CdIn1.9Sn0.1S4The 3d XPS map of middle Sn；
Fig. 4 is CdIn2-xSnxS4(x=0,0.05,0.1) the UV-Vis-NIR absorption spectrum of series of samples；
Fig. 5 is that Sn adulterates CdIn2S4Band structure map afterwards.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail and completely, but the present invention is limited to absolutely not embodiment.
Embodiment 1CdIn2-xSnxS4(x=0,0.05,0.1) preparation of material
By Cd powder (purity 99.99%), In (purity 99.999%), S powder (purity 99.999%) and Sn powder
(purity 99.99%) is according to CdIn2-xSnxS4The stoichiometric ratio of (x=0,0.05,0.1) weighs, and is put into quartz glass tube
In, and the effective oxyhydrogen flame of quartz glass is sealed；The quartz glass tube of sealing is put into temperature programmed control Muffle furnace, with 2 DEG C/minute
Clock rate rate is to slowly warm up to 750 DEG C and cools to room temperature with the furnace after keeping the temperature 24 hours；Again after open pipe, gained sample is placed in agate
It is ground in mortar, Vacuum Package is slowly heated up in quartz glass tube, being placed in temperature programmed control Muffle furnace with 2 DEG C/min of rates
It is sintered and keeps the temperature again 48 hours to 750 DEG C, sample cools to room temperature with the furnace, regrinds after open pipe to obtain the final product.
Embodiment 2CdIn2-xSnxS4(x=0,0.05,0.1) preparation of material
The binary compound of Cd, In, S and Sn by purity not less than 99.99% are according to CdIn2-xSnxS4(x=0,0.05,
0.1) stoichiometric ratio weighs, and is put into quartz glass tube, and the effective oxyhydrogen flame of quartz glass is sealed；By the stone of sealing
English glass tube is put into temperature programmed control Muffle furnace, with furnace after being to slowly warm up to 700 DEG C with 5 DEG C/min of rates and kept the temperature 48 hours
It is cooled to room temperature；Again after open pipe, gained sample being placed in agate mortar and is ground, Vacuum Package is placed in quartz glass tube, in
In temperature programmed control Muffle furnace, then 700 DEG C being to slowly warm up to 5 DEG C/min of rates and is sintered and keeps the temperature again 24 hours, sample is with furnace
It is cooled to room temperature, is regrind after open pipe to obtain the final product.
Embodiment 3CdIn2-xSnxS4(x=0,0.05,0.1) preparation of material
By Cd powder (purity 99.99%), In (purity 99.999%), S powder (purity 99.999%) and Sn powder
(purity 99.99%) is according to CdIn2-xSnxS4The stoichiometric ratio of (x=0,0.05,0.1) weighs, and is put into quartz glass tube
In, and the effective oxyhydrogen flame of quartz glass is sealed；The quartz glass tube of sealing is put into temperature programmed control Muffle furnace, with 3 DEG C/minute
Clock rate rate is to slowly warm up to 750 DEG C and cools to room temperature with the furnace after keeping the temperature 24 hours；Again after open pipe, gained sample is placed in agate
It is ground in mortar, Vacuum Package is placed in quartz glass tube, is slowly risen in temperature programmed control Muffle furnace, then with 3 DEG C/min of rates
Temperature is sintered and is kept the temperature 24 hours again to 800 DEG C, and sample cools to room temperature with the furnace, regrinds after open pipe to obtain the final product.
Embodiment 4CdIn2-xSnxS4(x=0,0.05,0.1) preparation of material
By Cd powder (purity 99.99%), In (purity 99.999%), S powder (purity 99.999%) and Sn powder
(purity 99.99%) is according to CdIn2-xSnxS4The stoichiometric ratio of (x=0,0.05,0.1) weighs, and is put into quartz glass tube
In, and the effective oxyhydrogen flame of quartz glass is sealed；The quartz glass tube of sealing is put into temperature programmed control Muffle furnace, with 4 DEG C/minute
Clock rate rate is to slowly warm up to 800 DEG C and cools to room temperature with the furnace after keeping the temperature 24 hours；Again after open pipe, gained sample is ground in agate
It is ground in alms bowl, Vacuum Package slowly rises in quartz glass tube, being placed in temperature programmed control Muffle furnace, then with 4 DEG C/min of rates
Temperature is sintered and is kept the temperature 24 hours again to 800 DEG C, and sample cools to room temperature with the furnace, target powder sample is obtained after open pipe, again
Grinding.
Embodiment 5CdIn2-xSnxS4(x=0,0.05,0.1) preparation of material
The binary compound of Cd, In, S and Sn by purity not less than 99.99% are according to CdIn2-xSnxS4(x=0,0.05,
0.1) stoichiometric ratio weighs, and is put into quartz glass tube, and the effective oxyhydrogen flame of quartz glass is sealed；By the stone of sealing
English glass tube is put into temperature programmed control Muffle furnace, with furnace after being to slowly warm up to 780 DEG C with 5 DEG C/min of rates and kept the temperature 36 hours
It is cooled to room temperature；Again after open pipe, gained sample is ground in agate mortar, Vacuum Package is placed in journey in quartz glass tube
In sequence temperature control Muffle furnace, then 800 DEG C being to slowly warm up to 5 DEG C/min of rates and is sintered and keeps the temperature again 24 hours, sample is cold with furnace
But it to room temperature, is regrind after open pipe to obtain the final product.
CdIn in effect example embodiment 12-xSnxS4(x=0,0.05,0.1) test and characterization of material
To the doping CdIn in embodiment 12S4Semiconductor structure, elemental analysis, Determination of Different Valence States and ultraviolet-visible-are close red
Outer absorption spectrum carries out analysis test, and the results are shown in attached figure 1-5, wherein structure is characterized using X ray diffracting spectrum, elemental analysis
It is measured using energy disperse spectroscopy, Determination of Different Valence States is characterized using photoelectron spectroscopy, and UV-visible-near infrared absorption is in Hitachi
It is measured on U4100 UV-Vis-NIR spectrophotometer.
Referring to attached drawing 1, CdIn2-xSnxS4(x=0,0.05,0.1) XRD spectrum of series of samples can be seen that all diffraction
Peak is all corresponding with standard card, illustrates that prepared sample is pure phase.
Referring to attached drawing 2, CdIn1.9Sn0.1S4EDX elemental analysis atlas analysis it is found that sample by tetra- kinds of Cd, In, S and Sn
Element composition.
Referring to attached drawing 3, CdIn is selected1.9Sn0.1S4Sample carries out XPS analysis test, as a result further confirm that sample by Cd,
Tetra- kinds of element compositions of In, S and Sn；Attached drawing 3 is the 3d spectrogram of Sn element, by being fitted XPS spectrum figure, Sn 3d5/2Peak is segmented into
Two peaks, are located at 486.3eV and 487.0eV；Sn 3d3/2Also two peaks are segmented into, be located at 495.3eV and
495.5eV；XPS analysis may infer that Sn element exists in two forms in compound, respectively Sn2+And Sn4+。
It is CdIn referring to attached drawing 42-xSnxS4The UV-Vis-NIR absorption spectrum of sample, it can be seen that after Sn doping
It can observe two ABSORPTION EDGEs, verify the optical absorption ability of its enhancing；Wherein the absorption curve of Sn doped samples first from
1350nm (1.09eV) nearby starts to increase, and reaches first platform in 700nm (1.77eV), then from 630nm (2.06eV)
Nearby start influx and translocation again, second ABSORPTION EDGE occurs.
Referring to attached drawing 5, CdIn is adulterated for Sn2S4Band structure map afterwards, it can be seen that after Sn doping, in conduction band
Bottom introduces a new energy band, which is made of the energy level of two Spin Splittings, and fermi level passes through the energy band, says
Phaneroplasm system has metallicity, increases by one and absorbs originating from transition of the electronics from valence band to Intermediate Gray.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention are fallen within the scope of the claimed invention.
Claims (7)
1. a kind of enhancing CdIn2S4The method of optical absorption, which is characterized in that in semiconductor CdIn2S4Middle doping nontransition metal
Atom Sn induces CdIn2S4Band gap in generate interstitial impurity energy band, wherein doping position be taken with nontransition metal atom Sn
For the semiconductor CdIn2S4Middle part In atom, the chemical molecular formula of products therefrom are CdIn2-xSnxS4, 0 < x < 2 in formula, packet
Include following steps:
S1, according to the CdIn2-xSnxS4Stoichiometric ratio weigh Cd, In, S and Sn raw material, Vacuum Package is in quartz glass tube
In；
S2, quartz glass tube described in step S1 is placed in temperature programmed control Muffle furnace, is slowly risen with 2-5 DEG C/min of rate
Temperature is to 700-800 DEG C of reaction-sintered, furnace cooling after heat preservation 24-48 hours；
S3, product after cooling described in step S2 is poured out and is ground, Vacuum Package is placed in in quartz glass tube again
In temperature programmed control Muffle furnace, then 700-800 DEG C of reaction-sintered be to slowly warm up to 2-5 DEG C/min of rate, keep the temperature 24-48 hours
It is regrind after furnace cooling afterwards.
2. a kind of enhancing CdIn as described in claim 12S4The method of optical absorption, which is characterized in that described in step S1
Cd, In, S and Sn raw material include simple substance or binary compound, and purity is not less than 99.99%.
3. a kind of enhancing CdIn as described in claim 12S4The method of optical absorption, which is characterized in that the interstitial impurity
Energy band has metallicity.
4. a kind of enhancing CdIn as claimed in claim 32S4The method of optical absorption, which is characterized in that the interstitial impurity
Energy band is formed by Sn-5s state and S-3p state hydridization.
5. a kind of enhancing CdIn as described in claim 12S4The method of optical absorption, which is characterized in that the non-transition gold
The doping content for belonging to atom Sn optimization is not more than 5at%.
6. a kind of doping CdIn2S4Semiconductor, which is characterized in that pass through the described in any item enhancing CdIn of claim 1-52S4Light
The method absorbed is learned to obtain.
7. a kind of doping CdIn as claimed in claim 62S4Semiconductor, which is characterized in that chemical molecular formula CdIn2- xSnxS4, wherein 0 < x < 2.
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| DE2850930A1 (en) * | 1978-11-24 | 1980-06-19 | Siemens Ag | Light detector with sensitivity max. at helium-neon laser wavelength - has cadmium indium sulphide spinel body and metal-semiconductor junction |
| CN102101055A (en) * | 2011-01-31 | 2011-06-22 | 黑龙江省科学院石油化学研究院 | Method for preparing transition metal ion-doped porous CdIn2S4 photocatalyst |
| CN106784067A (en) * | 2016-12-14 | 2017-05-31 | 上海电机学院 | A kind of wide spectrum solar absorption semiconductor and preparation method thereof |
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| US20100276731A1 (en) * | 2009-05-04 | 2010-11-04 | Brookhaven Science Associates, Llc. | Inorganic Nanocrystal Bulk Heterojunctions |
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| DE2850930A1 (en) * | 1978-11-24 | 1980-06-19 | Siemens Ag | Light detector with sensitivity max. at helium-neon laser wavelength - has cadmium indium sulphide spinel body and metal-semiconductor junction |
| CN102101055A (en) * | 2011-01-31 | 2011-06-22 | 黑龙江省科学院石油化学研究院 | Method for preparing transition metal ion-doped porous CdIn2S4 photocatalyst |
| CN106784067A (en) * | 2016-12-14 | 2017-05-31 | 上海电机学院 | A kind of wide spectrum solar absorption semiconductor and preparation method thereof |
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| E. S. R. investigations on chromium doped CdIn2S4;J.C.M. Henning 等;《Physics Letters A》;19691103;第30卷(第5期);全文 |
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